CN106750545A - A kind of zinc stearate/graphene oxide composite material and preparation method thereof - Google Patents
A kind of zinc stearate/graphene oxide composite material and preparation method thereof Download PDFInfo
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- CN106750545A CN106750545A CN201710020152.1A CN201710020152A CN106750545A CN 106750545 A CN106750545 A CN 106750545A CN 201710020152 A CN201710020152 A CN 201710020152A CN 106750545 A CN106750545 A CN 106750545A
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- graphene oxide
- zinc stearate
- zinc
- composite material
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 title claims abstract description 151
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 144
- 239000002131 composite material Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims description 22
- 239000011701 zinc Substances 0.000 claims description 41
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 40
- 229910052725 zinc Inorganic materials 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 239000002904 solvent Substances 0.000 claims description 25
- 239000006185 dispersion Substances 0.000 claims description 24
- 235000021355 Stearic acid Nutrition 0.000 claims description 23
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 23
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 23
- 239000008117 stearic acid Substances 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 18
- 239000003960 organic solvent Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 10
- 239000004246 zinc acetate Substances 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 6
- 229960001763 zinc sulfate Drugs 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- 239000005060 rubber Substances 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- RXBXBWBHKPGHIB-UHFFFAOYSA-L zinc;diperchlorate Chemical compound [Zn+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O RXBXBWBHKPGHIB-UHFFFAOYSA-L 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- 230000003466 anti-cipated effect Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 4
- XIVNZHXRIPJOIZ-UHFFFAOYSA-N octadecanoic acid;zinc Chemical compound [Zn].CCCCCCCCCCCCCCCCCC(O)=O XIVNZHXRIPJOIZ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 51
- 239000000047 product Substances 0.000 description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 26
- 238000000034 method Methods 0.000 description 26
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 20
- 239000004800 polyvinyl chloride Substances 0.000 description 14
- 229920000915 polyvinyl chloride Polymers 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- KYIDJMYDIPHNJS-UHFFFAOYSA-N ethanol;octadecanoic acid Chemical compound CCO.CCCCCCCCCCCCCCCCCC(O)=O KYIDJMYDIPHNJS-UHFFFAOYSA-N 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 8
- 239000004033 plastic Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 description 6
- 238000013019 agitation Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000012760 heat stabilizer Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 238000005253 cladding Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000007500 overflow downdraw method Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 238000012805 post-processing Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 1
- 239000001293 FEMA 3089 Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007033 dehydrochlorination reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000000346 nonvolatile oil Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229940095696 soap product Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- IPCXNCATNBAPKW-UHFFFAOYSA-N zinc;hydrate Chemical compound O.[Zn] IPCXNCATNBAPKW-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention provides a kind of zinc stearate/graphene oxide composite material, including zinc stearate and the graphene oxide for being compounded in zinc stearate surface.With graphene oxide be combined zinc stearate by the present invention, the sheet zinc stearate composite of micron level is obtained, size is homogeneous, regular appearance, graphene oxide is coated on zinc stearate surface by chemical bond, formed graphene oxide coat stearic acid zinc metal sheet clad structure, or " zinc stearate Graphene zinc stearate " stratiform overlaying structure, the present invention provide zinc stearate/graphene oxide composite material there is more preferable heat endurance and lubricity.
Description
Technical field
It is multiple the invention belongs to zinc stearate technical field of composite materials, more particularly to a kind of zinc stearate/graphene oxide
Condensation material and preparation method thereof.
Background technology
Zinc stearate (Zinc stearate), also known as zinc octadecanate or Stearic Acid zinc, molecular formula is C36H70O4Zn, molecule
It is 632.33 to measure, and white powder is water insoluble, is dissolved in the organic solvents such as ethanol, benzene, toluene or the turpentine oil of heat；Run into acid point
Solution is into stearic acid and corresponding salt；Have fire danger under the dry condition, there is hygroscopicity under humidified condition.It is commonly divided into
Solidity zinc stearate and water-based zinc stearate.
The production method of zinc stearate has two kinds：Water law and fusion method.As a rule, the aobvious acid of the zinc stearate of water law production
Property, melting Faxian alkalescence.Water law under conditions of water is medium, adds catalyst also known as wet method, controls certain temperature, pressure
Power, is subsequently adding metal hydroxides, is replaced onto catalyst metal ion by catalyst, then by catalyst in itself
Replace on stearic acid again, so as to reach the purpose of generation slaine.Fusion method, also known as dry method, refers to the bar existed in catalyst
Under part, metal oxide (zinc oxide) is directly added into the stearic acid of melting, controls certain temperature, pressure and mixing speed,
Stearate is obtained by reaction.
The class that zinc stearate is used in many polymer has the additive of various functions, various based on its uniqueness
The physicochemical property of change, many key areas such as plastics, coating, lubricating grease, weaving, building, papermaking, pigment obtain extensively and
Important application, and constantly there is new application approach to be developed, its main application fields is coating, plastics and rubber
Industry；Heat stabilizer, lubricant, lubricating grease, accelerator or thickener such as can be used as in resin art, usually as PVC trees
Fat heat stabilizer.PVC (polyvinyl chloride) is to be only second to one of most wide plastics of polyethylene consumption maximum, purposes in the world at present,
And wide market has been won with the performance such as its fire-retardant, insulation, wear-resistant.Polyvinyl chloride resin and its product are lacked due to the structure of itself
Fall into, there is easy thermal degradation and aging, more than 160 DEG C of its processing temperature is also higher than 120 DEG C of decomposition temperature；Therefore,
PVC will be become into product, heat stabilizer must be just added during machine-shaping, to delay or prevent the heat of polyvinyl chloride resin
Degraded, and the main cause of polyvinyl chloride heat ageing is exactly to be sloughed small molecule by thermal decomposition, on the one hand zinc stearate can capture
The hydrogen chloride for splitting away off, on the other hand can also replace present in chlorine atom in allyl chloride, generate more stable ester,
So as to eliminate the initiation source of dehydrochlorination in polymeric material.Therefore, zinc stearate is generally selected in field as PVC plastic
Heat stabilizer and lubricant.
In view of zinc stearate is further modified always in the important use of zinc stearate, industry, so as to improve
Its performance expands its application field, and the preparation technology of zinc stearate is also to limit its bottleneck for continuing to develop, stearic acid
The production technology of zinc is broadly divided into two kinds of double decomposition and fusion method, and double decomposition work is generally used in manufacturer at home
Skill.Raw material used in this method has the raw materials such as stearic acid, zinc sulfate, caustic soda, by after metathesis reaction, washing is dried,
Drying etc. some row techniques finally obtain finished product.Although its reaction condition is gentle, by controlling reaction temperature, etc. technique bar
Part, can obtain the metallic soap product that color and luster is good, purity is higher, but its own has inevitable defect -- and production capacity is low and energy
Consumption is high, and such as reaction mass is liquid-solid than high, low production efficiency；Need to consume a large amount of water and washed, amplification quantity saliferous and press from both sides side by side
Waste water with organic matter；Energy consumption for drying is big, and product apparent density is small, and dust from flying is serious；More importantly double decomposition life
The zinc stearate of product shows very poor transparency in coating, it is impossible to be used widely.
Therefore, a kind of modified zinc stearate material with more preferable performance how is obtained, tradition can also be especially solved
Defect in preparation method, it has also become many line R＆D and production personnel and urgently to be resolved hurrily important of manufacturer is asked in the industry in industry
Topic.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of zinc stearate/graphene oxide composite wood
Material and preparation method thereof, zinc stearate/graphene oxide composite material that the present invention is provided has preferable heat endurance, and
Preparation method process is simple, mild condition, safety and environmental protection is adapted to large-scale industrial production.
The invention provides a kind of zinc stearate/graphene oxide composite material, including zinc stearate and it is compounded in tristearin
The graphene oxide of sour zinc surface.
Preferably, the zinc stearate is sheet zinc stearate；
The thickness of the graphene oxide is 0.1~0.5nm；
The zinc stearate is 1000 with the mass ratio of the graphene oxide：(1~50).
Preferably, the piece footpath of the zinc stearate/graphene oxide composite material is 4~12 μm；
The thickness of the zinc stearate/graphene oxide composite material is 30~70nm.
The invention provides a kind of preparation method of zinc stearate/graphene oxide composite material, comprise the following steps：
A) by graphene oxide, organic solvent miscible with water and water by after dispersion, obtaining graphene oxide dispersion
Liquid；
B after the graphene oxide dispersion for) obtaining above-mentioned steps and the mixing of zinc source, precursor solution is obtained；
C) precursor solution for obtaining above-mentioned steps obtains zinc stearate/graphene oxide after being reacted with stearic acid
Composite.
Preferably, in the graphene oxide dispersion, the mass fraction of graphene oxide is 0.5 ‰~5 ‰；
The organic solvent miscible with water includes that alcohols solvent, amine solvent, ketones solvent and high molecular polymer are molten
One or more in agent；
The mass ratio of the organic solvent miscible with water and water is (0.01~1)：1.
Preferably, the zinc source is zinc source solution；
The concentration of zinc source solution is 0.01~0.5mol/L；
The zinc source includes one or more in zinc acetate, zinc chloride, zinc nitrate, zinc sulfate and zinc perchlorate；
The graphene oxide is 1 with the mass ratio of zinc ion in the zinc source：(1~10).
Preferably, it is described to be mixed into ultrasonic disperse；
The temperature of the mixing is 20~60 DEG C；The time of the mixing is 10~60min.
Preferably, the step C) it is specially：
To stearic acid organic solution is slowly added in the precursor solution that above-mentioned steps are obtained, tristearin is obtained after being reacted
Sour zinc/graphene oxide composite material；
The stearic acid is (1.5~2.5) with the mol ratio of zinc ion in the zinc source：1；
The temperature of the reaction is 60~100 DEG C；The time of the reaction is 90~150min.
Preferably, the concentration of the stearic acid organic solution is 0.1~0.3mol/L；
Solvent in the stearic acid organic solution includes that alcohols solvent, benzene kind solvent, polynary alkanes solvent and ethers are molten
One or more in agent；
The speed being slowly added to is 0.3~0.7mL/s.
Present invention also offers the zinc stearate/graphene oxide composite material described in above-mentioned technical proposal any one or
Zinc stearate/graphene oxide composite material prepared by above-mentioned technical proposal any one is led in rubber or resin additive
Application in domain.
The invention provides a kind of zinc stearate/graphene oxide composite material, including zinc stearate and it is compounded in tristearin
The graphene oxide of sour zinc surface.Compared with prior art, the present invention is further for the performance need of existing zinc stearate
The present situation of lifting, zinc stearate is combined with graphene oxide, has obtained the sheet zinc stearate composite wood of micron level
Material, size is homogeneous, regular appearance, and graphene oxide is coated on zinc stearate surface by chemical bond, forms graphite oxide
Alkene coat stearic acid zinc metal sheet clad structure, or " zinc stearate-Graphene-zinc stearate " stratiform overlaying structure, this hair
Zinc stearate/the graphene oxide composite material of bright offer has more preferable heat endurance and lubricity.Test result indicate that, this
Invent the zinc stearate/graphene oxide composite material for preparing and compare common zinc stearate, thermal stability is improved and reached
116%.
Brief description of the drawings
Fig. 1 is the process flow diagram that the embodiment of the present invention 1 prepares zinc stearate/graphene oxide composite material；
Fig. 2 is the XRD x ray diffraction collection of illustrative plates of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention；
Fig. 3 is that the SEM of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention 1 is shone
Piece；
Fig. 4 is that the SEM of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention 2 is shone
Piece；
Fig. 5 is the electron scanning micrograph of conventional zinc stearate；
Fig. 6 is that the SEM of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention 3 is shone
Piece.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but
It should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention, rather than to invention claim
Limitation.
The all raw materials of the present invention, originate to it and are not particularly limited, commercially buying or according to people in the art
Known to member prepared by conventional method.
The all raw materials of the present invention, are not particularly limited to its purity, present invention preferably employs analyze pure or zinc stearate and
The conventional purity used in graphene oxide field.
The invention provides a kind of zinc stearate/graphene oxide composite material, including zinc stearate and it is compounded in tristearin
The graphene oxide of sour zinc surface.
The present invention is not particularly limited to the zinc stearate, is with zinc stearate material well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, combining case and properties of product
The bright zinc stearate material is preferably sheet zinc stearate material.The present invention is not particularly limited to the graphene oxide,
With graphene oxide composite material well known to those skilled in the art, those skilled in the art can according to practical condition,
Combining case and properties of product are selected and are adjusted material.
The present invention is not particularly limited to the size dimension of the zinc stearate/graphene oxide composite material, with ability
The size dimension of zinc stearate composite known to field technique personnel, those skilled in the art can be according to actual production
Situation, combining case and properties of product are selected and adjusted, zinc stearate/graphene oxide composite material of the present invention
Piece footpath be preferably 4~12 μm, most preferably more preferably 6~10 μm, 7~9 μm；Zinc stearate of the present invention/oxidation stone
The thickness of black alkene composite is preferably 30~70nm, most preferably more preferably 40~60nm, 45~55nm.
The present invention is to the actual conditions of the graphene oxide layer of the zinc stearate/graphene oxide composite material without spy
Do not limit, those skilled in the art can be selected and be adjusted according to practical condition, combining case and properties of product,
The thickness of graphene oxide of the present invention be preferably 0.1~0.5nm, more preferably 0.2~0.4nm, most preferably 0.25~
0.35nm。
The present invention is not particularly limited to the mass ratio of the zinc stearate/graphene oxide composite material, this area skill
Art personnel can be selected and be adjusted according to practical condition, combining case and properties of product, tristearin of the present invention
Sour zinc is preferably 1000 with the mass ratio of the graphene oxide：(1~50), more preferably 1000：(5~40), most preferably
1000：(15~30).
The present invention is not particularly limited to described being combined, with composite definitions well known to those skilled in the art, this hair
Bright to be preferably cladding, half cladding, stacking, deposition, doping or grow, more preferably cladding, half coat or are laminated, and most preferably wrap
Cover or be laminated.The present invention is not particularly limited to the cladding and stacking, with cladding well known to those skilled in the art and stacking
Definition, those skilled in the art can be selected and be adjusted according to practical condition, combining case and properties of product
It is whole.
The invention provides a kind of preparation method of zinc stearate/graphene oxide composite material, comprise the following steps：
A) by graphene oxide, organic solvent miscible with water and water by after dispersion, obtaining graphene oxide dispersion
Liquid；
B after the graphene oxide dispersion for) obtaining above-mentioned steps and the mixing of zinc source, precursor solution is obtained；
C) precursor solution for obtaining above-mentioned steps obtains zinc stearate/graphene oxide after being reacted with stearic acid
Composite.
Graphene oxide, organic solvent miscible with water and water are aoxidized stone by the present invention by after dispersion, obtaining first
Black alkene dispersion liquid.
The present invention is not particularly limited to the graphene oxide, is with graphene oxide well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted according to practical condition, combining case and properties of product；This hair
The bright source to the graphene oxide is not particularly limited, and is prepared with preparation method well known to those skilled in the art or commercially available
Purchase, those skilled in the art can be selected and be adjusted according to practical condition, combining case and properties of product
It is whole.
The present invention is not particularly limited to the organic solvent miscible with water, with well known to those skilled in the art and water
The organic solvent for dissolving each other, those skilled in the art can enter according to practical condition, combining case and properties of product
Row selection and adjust, organic solvent miscible with water of the present invention preferably include alcohols solvent, amine solvent, ketones solvent and
One or more in high molecular polymer solvent, more preferably ethanol, acetone, toluene or ether, most preferably ethanol.
The present invention is not particularly limited to the addition of the organic solvent miscible with water, ripe with those skilled in the art
The conventional proportions known, those skilled in the art can be carried out according to practical condition, combining case and properties of product
The mass ratio of selection and adjustment, organic solvent miscible with water of the present invention and water is preferably (0.01~1)：1, more preferably
(0.1~0.9)：1, more preferably (0.3~0.7)：1, most preferably (0.4~0.6)：1.The present invention is to the graphene oxide
Addition be not particularly limited, those skilled in the art can be according to practical condition, combining case and properties of product
Being selected and adjusted, in graphene oxide dispersion of the present invention, the mass fraction of graphene oxide is preferably 0.5 ‰~
5 ‰, more preferably 1 ‰~4 ‰, most preferably 2 ‰~3 ‰.
The present invention is not particularly limited to the scattered mode, is with process for dispersing well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, combining case and properties of product
The bright dispersion is preferably ultrasonic disperse.The present invention is not particularly limited to the scattered time, with those skilled in the art
Well known jitter time, those skilled in the art can enter according to practical condition, combining case and properties of product
Row selection and adjustment, the scattered time of the present invention are preferably 10~40min, more preferably 15~35min, most preferably 20
~30min.The present invention is not particularly limited to the scattered frequency, is with dispersion frequency well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, combining case and properties of product
The bright scattered frequency is preferably 20~80KHz, most preferably more preferably 30~60KHz, 40~50KHz.
Above-mentioned steps of the present invention have obtained graphene oxide two phase dispersant liquids in water and organic solvent, then aoxidize this
After graphene dispersing solution and the mixing of zinc source, precursor solution is obtained.
The present invention is not particularly limited to the zinc source, with zinc source well known to those skilled in the art, this area skill
Art personnel can be selected and be adjusted according to practical condition, product requirement and quality requirement, and zinc source of the present invention is excellent
Choosing includes one or more in zinc acetate, zinc chloride, zinc nitrate, zinc sulfate and zinc perchlorate, more preferably zinc acetate, chlorination
Zinc, zinc nitrate, zinc sulfate or zinc perchlorate, most preferably zinc acetate.The present invention is to the additional proportion in the zinc source without special
Limitation, those skilled in the art can be selected and be adjusted, this hair according to practical condition, product requirement and quality requirement
The bright graphene oxide is preferably 1 with the mass ratio of zinc ion in the zinc source：(1~10), more preferably 1：(3~8), most
Preferably 1：(4~7).Further to improve mixed effect and the reaction effect in later stage, the zinc source is preferably zinc to the present invention
Source solution.The present invention is not particularly limited to the concentration of zinc source solution, with normal concentration well known to those skilled in the art
, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, this
The concentration for inventing zinc source solution is preferably 0.01~0.5mol/L, more preferably 0.05~0.4mol/L, most preferably 0.1
~0.3mol/L.
The present invention mixes scattered effect and the reaction effect in later stage, the step B to be further ensured that) it is preferably upwards
Stating after be added dropwise in the graphene oxide dispersion that step is obtained the mixing of zinc source, obtaining precursor solution.The present invention is to the dropwise addition
Speed be not particularly limited, with rate of addition well known to those skilled in the art, those skilled in the art can basis
Practical condition, product requirement and quality requirement are selected and adjusted, and the speed of dropwise addition of the present invention is preferably 0.3~
0.7mL/s, more preferably 0.4~0.6mL/s, most preferably 0.45~0.55mL/s.
The present invention is not particularly limited to the temperature of the mixing, and the temperature with mixing well known to those skilled in the art is
Can, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, the present invention
The temperature of the mixing is preferably 20~60 DEG C, most preferably more preferably 30~50 DEG C, 35~45 DEG C.The present invention is to described mixed
The time of conjunction is not particularly limited, and with incorporation time well known to those skilled in the art, those skilled in the art can be with root
Selected and adjusted according to practical condition, product requirement and quality requirement, the time of mixing of the present invention is preferably 10
~60min, more preferably 20~50min, most preferably 30~40min.The present invention is not limited especially the mode of the mixing
System, with mixed method well known to those skilled in the art, those skilled in the art can be according to practical condition, product
It is required that and quality requirement selected and adjusted, it is of the present invention mixing be preferably ultrasonic disperse.The present invention is to the ultrasound point
Scattered frequency is not particularly limited, and with dispersion frequency well known to those skilled in the art, those skilled in the art can be with root
Selected and adjusted according to practical condition, product requirement and quality requirement, scattered frequency of the present invention is preferably 20
~80KHz, more preferably 30~60KHz, most preferably 40~50KHz.
The last precursor solution for obtaining above-mentioned steps of the invention obtains zinc stearate/oxygen after being reacted with stearic acid
Graphite alkene composite.
The present invention mixes scattered effect and the reaction effect in later stage, above-mentioned steps, i.e., described step to be further ensured that
C) it is preferably in the precursor solution obtained to above-mentioned steps and is slowly added to stearic acid organic solution, tristearin is obtained after being reacted
Sour zinc/graphene oxide composite material.
The present invention is not particularly limited to the solvent in the stearic acid organic solution, with well known to those skilled in the art
Conventional organic solvent, those skilled in the art can be selected according to practical condition, product requirement and quality requirement
Select and adjust, it is molten that the solvent in stearic acid organic solution of the present invention preferably includes alcohols solvent, benzene kind solvent, polynary alkanes
One or more in agent and ether solvent, more preferably ethanol, acetone, toluene or ether, most preferably ethanol；Specifically can be with
It is consistent with foregoing organic solvent miscible with water.The present invention is not particularly limited to the stearic addition, this area
Technical staff can be selected and be adjusted according to practical condition, product requirement and quality requirement, tristearin of the present invention
The sour mol ratio with zinc ion in the zinc source is (1.5~2.5)：1, more preferably (1.7~2.3)：1, most preferably (1.9
~2.1)：1.The present invention is not particularly limited to the concentration of the stearic acid organic solution, with well known to those skilled in the art
The concentration of conventional soln, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement
Selection and adjust, the concentration of stearic acid organic solution of the present invention is preferably 0.1~0.3mol/L, more preferably 0.15~
0.25mol/L, most preferably 0.17~0.23mol/L.
The present invention is not particularly limited to the speed being slowly added to, with rate of addition well known to those skilled in the art
, those skilled in the art can be selected and be adjusted, this hair according to practical condition, product requirement and quality requirement
It is slowly added to preferably instill described in bright, the speed of the instillation is preferably 0.3~0.7mL/s, more preferably 0.4~0.6mL/
S, most preferably 0.45~0.55mL/s.The present invention is not particularly limited to the condition of the reaction, and those skilled in the art can
Selected and adjusted with according to practical condition, product requirement and quality requirement, the temperature of reaction of the present invention is preferred
It is 60~100 DEG C, more preferably 70~90 DEG C, most preferably 75~85 DEG C；The time of the reaction is preferably 90~150min,
More preferably 100~140min, most preferably 110~130min.
The present invention goes back further to improve the performance of product and the integrality and operability of integrated artistic after the reaction
Including postprocessing working procedures.The present invention is not particularly limited to the postprocessing working procedures, with rear place well known to those skilled in the art
Science and engineering sequence, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement
It is whole, postprocessing working procedures of the present invention preferably include to separate, wash and dry in one or more, be more preferably followed successively by point
From, washing and dry.
The present invention is not particularly limited to the mode of the separation, is with separate mode well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, the present invention
The mode of the separation is preferably suction filtration；The present invention is not particularly limited to the mode of the washing, with those skilled in the art
Well known mode of washing, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement
Selection and adjustment, the mode of washing of the present invention is preferably washing and alcohol washes alternately multiple washing；The washing time
Number is preferably 2~5 times, more preferably 3~4 times.The present invention is not particularly limited to the dry mode, with art technology
Drying mode known to personnel, those skilled in the art can be according to practical condition, product requirement and quality requirement
Selected and adjusted, dry mode of the present invention is preferably vacuum drying；The dry temperature is preferably 40~70
DEG C, more preferably 45~65 DEG C, most preferably 50~60 DEG C.
The present invention for the zinc stearate that largely uses now for double decomposition i.e. fixed oil with caustic soda after saponification
Standby with zinc sulfate metathetical, granulation carries out zinc stearate synthesis after also having partial high pressure frit reaction, or uses wet-chemical
Method realizes the chemical synthesis of zinc stearate, there is complex operation, the problem that steps flow chart is cumbersome or production cost is higher.The present invention
Zinc stearate/graphene composite material is prepared using one-step synthesis chemical method, the double decomposition and fusion method of abandoning tradition are used
Improved wet chemistry method, has prepared zinc stearate/graphene oxide composite material, method letter under normal pressure, cryogenic conditions
It is single easy to operate, it is easy to which that prepared by scale, repeatability, the composite size for obtaining is homogeneous, and pattern is easily controllable, with good
Application prospect, and the controllable continuous preparation of zinc stearate is realized, and by the graphene coated of high-intensity high-tenacity on surface
Or stacking is compound, the dispersiveness and workability energy of composite are improve, heat endurance is contributed to after adding PVC as auxiliary agent
Improve.
Technical scheme also further can be preferably more common reaction raw materials, such as zinc acetate both reduced
Reactions steps, reduce synthesis cost again, meanwhile, also realize prepared by low-temperature atmosphere-pressure environment, the requirement to reaction environment is substantially reduced,
It is easy to scale, preparation of industrialization, does not use the contour harm reducing agent of hydrazine hydrate during simultaneous reactions, it is to avoid environmental pollution.
Present invention also offers the zinc stearate/graphene oxide composite material described in above-mentioned technical proposal any one or
Zinc stearate/graphene oxide composite material prepared by above-mentioned technical proposal any one is led in rubber or resin additive
Application in domain.
The present invention is not particularly limited to the resin, with resin well known to those skilled in the art, this area skill
Art personnel can be selected and be adjusted according to practical condition, product requirement and quality requirement, and resin of the present invention is excellent
Elect polyvinyl chloride resin as.The present invention is not particularly limited to the resin additive, is with resin additive well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, the present invention
The resin additive is preferably heat stabilizer and/or lubricant, more preferably heat stabilizer or lubricant.
Above-mentioned steps of the present invention provide a kind of zinc stearate/graphene oxide composite material and preparation method thereof, innovation
Property the step of use one chemistry method of formation prepare zinc stearate/graphene composite material, the composite is uniformly dispersed, and size is equal
One, wherein in the form of sheets, composite gauge is 5~10 μm to zinc stearate, and thickness is 20~50nm, and the material has special bag
Cover and stepped construction, in the field such as rubber and PVC plastic applications well prospect；And the present invention prepares the side of zinc stearate material
Method, it is to avoid use autoclave, realizes prepared by low-temperature atmosphere-pressure.It is of the invention further preferably to use zinc acetate as raw material, take
The crude zinc oxide materials of generation routine, in final reaction step preferably by the way of oil bath heating, make under normal pressure, cryogenic conditions
Standby zinc stearate/graphene composite material, effectively reduces energy consumption needed for reaction system, reduces step needed for reaction, improves product
Purity, improves the repeatability of composite, does not use catalyst, improves reaction conversion ratio, while reducing operation and reacting
Step, reduces production cost, while can realize prepared by extensive industrialization, repeatability is high；The present invention is in technical side simultaneously
The raw material with environmental hazard such as hydrazine hydrate, green pollution-free are not used during case.Test result indicate that, the present invention
Zinc stearate/the graphene oxide composite material of preparation compares common zinc stearate, and thermal stability is improved and reached 116%.
In order to further illustrate the present invention, the zinc stearate/graphene oxide for providing the present invention with reference to embodiments
Composite and preparation method thereof has been described in detail, but it is to be understood that these embodiments are with the technology of the present invention side
Implemented under premised on case, given detailed implementation method and specific operating process, simply to further illustrate this hair
Bright feature and advantage, rather than limiting to the claimed invention, protection scope of the present invention is also not necessarily limited to following realities
Apply example.
Embodiment 1
The present embodiment prepares zinc stearate/graphene composite material by following steps：
First, graphene solution prepared by Hummers methods is dissolved in (Graphene matter in the mixed liquor of deionized water and ethanol
For 0.5, ‰) (ethanol and water volume ratio are 1 to amount fraction:1), ultrasound and stir 20min and obtain graphene dispersion solution under normal temperature；
2nd, the aqueous zinc acetate solution of 0.1mol/L is prepared, magnetic agitation obtains acetic acid zinc solution to state is clarified under normal temperature；
3rd, the stearic acid ethanol solution of 0.2mol/L is prepared, magnetic agitation obtains stearic acid ethanol to state is clarified under normal temperature
Solution；
4th, to the acetic acid zinc solution that (0.5mL/s) step 2 is slowly added dropwise in the GO dispersion solns obtained in step one, after
Continual ultrasonic and 30min is stirred at 40 DEG C, obtain precursor solution；
5th, it is molten to the stearic acid ethanol that (0.3mL/s) step 3 is slowly added dropwise in the precursor solution obtained in step 4
Liquid, after be transferred to oil bath, condensing reflux reaction 120min, obtains gray precipitate under the conditions of being kept for 80 DEG C；
6th, the separation of gray precipitate suction filtration will be obtained in step 5, after ultra-pure water and ethanol wash 3 times respectively, 50 DEG C of vacuum
Dry, obtain zinc stearate/graphene oxide composite material.
Referring to Fig. 1, Fig. 1 is the technological process letter that the embodiment of the present invention 1 prepares zinc stearate/graphene oxide composite material
Figure.
Material structure analysis is carried out to zinc stearate/graphene oxide composite material prepared by above-mentioned steps of the present invention.
Referring to Fig. 2, Fig. 2 is that the XRD rays of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention spread out
Penetrate collection of illustrative plates.As shown in Figure 2, the present invention has successfully prepared zinc stearate/graphene oxide composite material.
Referring to Fig. 3, Fig. 3 is the scanning electron of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention 1
Microphotograph.
From the figure 3, it may be seen that zinc stearate slabbing, size at 10 μm or so, the thickness of nanometer sheet in 50nm or so, in sheet
The Surface coating of zinc stearate has one layer of graphene oxide, forms zinc stearate/graphene oxide composite material, composite point
Dissipate uniform, size uniformity.
Material property analysis is carried out to zinc stearate/graphene oxide composite material prepared by above-mentioned steps of the present invention, will
Pure zinc stearate and zinc stearate/graphene oxide composite material be separately added into injection moulding in PVC plastic (zinc stearate and its
2%) composite addition is.
Referring to table 1, table 1 is zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention and common tristearin
The performance table of comparisons of sour zinc.
Embodiment 2
The present embodiment prepares zinc stearate/graphene composite material by following steps：
First, graphene solution prepared by Hummers methods is dissolved in (Graphene matter in the mixed liquor of deionized water and ethanol
For 1, ‰) (ethanol and water volume ratio are 1 to amount fraction:1), ultrasound and stir 20min and obtain graphene dispersion solution under normal temperature；
2nd, the aqueous zinc acetate solution of 0.15mol/L is prepared, magnetic agitation obtains acetic acid zinc solution to state is clarified under normal temperature；
3rd, the stearic acid ethanol solution of 0.3mol/L is prepared, magnetic agitation obtains stearic acid ethanol to state is clarified under normal temperature
Solution；
4th, to the acetic acid zinc solution that (0.5mL/s) step 2 is slowly added dropwise in the GO dispersion solns obtained in step one, after
Continual ultrasonic and 30min is stirred at 40 DEG C, obtain precursor solution；
5th, it is molten to the stearic acid ethanol that (0.3mL/s) step 3 is slowly added dropwise in the precursor solution obtained in step 4
Liquid, after be transferred to oil bath, condensing reflux reaction 120min, obtains gray precipitate under the conditions of being kept for 70 DEG C；
6th, the separation of gray precipitate suction filtration will be obtained in step 5, after ultra-pure water and ethanol wash 3 times respectively, 50 DEG C of vacuum
Dry, obtain zinc stearate/graphene composite material.
Material structure analysis is carried out to zinc stearate/graphene oxide composite material prepared by above-mentioned steps of the present invention.
Referring to Fig. 2, Fig. 2 is that the XRD rays of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention spread out
Penetrate collection of illustrative plates.As shown in Figure 2, the present invention has successfully prepared zinc stearate/graphene oxide composite material.
Referring to Fig. 4, Fig. 4 is the scanning electron of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention 2
Microphotograph.Referring to Fig. 5, Fig. 5 is the electron scanning micrograph of conventional zinc stearate.Can by Fig. 4 and Fig. 5 contrasts
Know, zinc stearate slabbing, size at 10 μm or so, the thickness of nanometer sheet in 20nm or so, on the surface of sheet zinc stearate
One layer of graphene oxide is coated with, zinc stearate/graphene composite material is formed, composite is uniformly dispersed, size uniformity, phase
Than conventional sheet zinc stearate, top layer is compounded with that accordion graphene oxide layer is thicker, and piece footpath is smaller, it may be possible to based on oxygen
As the core of growth in situ after the addition of graphite alkene, two sides growth zinc stearate, therefore the lamella of composite is thickening.
Material property analysis is carried out to zinc stearate/graphene oxide composite material prepared by above-mentioned steps of the present invention, will
Pure zinc stearate and zinc stearate/graphene oxide composite material be separately added into injection moulding in PVC plastic (zinc stearate and its
2%) composite addition is.
Referring to table 1, table 1 is zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention and common tristearin
The performance table of comparisons of sour zinc.
Embodiment 3
The present embodiment prepares zinc stearate/graphene composite material by following steps：
First, (Graphene mass fraction is in graphene solution prepared by Hummers methods being dissolved in into deionized water
0.5 ‰), ultrasound and stirs 20min and obtains graphene dispersion solution under normal temperature；
2nd, the aqueous zinc acetate solution of 0.2mol/L is prepared, magnetic agitation obtains acetic acid zinc solution to state is clarified under normal temperature；
3rd, the stearic acid ethanol solution of 0.4mol/L is prepared, magnetic agitation obtains stearic acid ethanol to state is clarified under normal temperature
Solution；
4th, to the acetic acid zinc solution that (0.5mL/s) step 2 is slowly added dropwise in the GO dispersion solns obtained in step one, after
Continual ultrasonic and 30min is stirred at 40 DEG C, obtain precursor solution；
5th, it is molten to the stearic acid ethanol that (0.3mL/s) step 3 is slowly added dropwise in the precursor solution obtained in step 4
Liquid, after be transferred to oil bath, condensing reflux reaction 90min, obtains gray precipitate under the conditions of being kept for 80 DEG C；
6th, the separation of gray precipitate suction filtration will be obtained in step 5, after ultra-pure water and ethanol wash 3 times respectively, 50 DEG C of vacuum
Dry, obtain zinc stearate/graphene composite material.
Material structure analysis is carried out to zinc stearate/graphene oxide composite material prepared by above-mentioned steps of the present invention.
Referring to Fig. 2, Fig. 2 is that the XRD rays of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention spread out
Penetrate collection of illustrative plates.As shown in Figure 2, the present invention has successfully prepared zinc stearate/graphene oxide composite material.
Referring to Fig. 6, Fig. 6 is the scanning electron of zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention 3
Microphotograph.It will be appreciated from fig. 6 that zinc stearate slabbing, size at 10 μm or so, the thickness of nanometer sheet in 20nm or so,
The Surface coating of sheet zinc stearate has one layer of graphene oxide, forms zinc stearate/graphene oxide composite material, composite wood
Material is uniformly dispersed, size uniformity.
Material property analysis is carried out to zinc stearate/graphene oxide composite material prepared by above-mentioned steps of the present invention, will
Pure zinc stearate and zinc stearate/graphene oxide composite material be separately added into injection moulding in PVC plastic (zinc stearate and its
2%) composite addition is.
Referring to table 1, table 1 is zinc stearate/graphene oxide composite material prepared by the embodiment of the present invention and common tristearin
The performance table of comparisons of sour zinc.
Zinc stearate/graphene oxide composite material and the performance of common zinc stearate prepared by the embodiment of the present invention of table 1
The table of comparisons
| Sample name | Heat-stable time (min) is pure | Heat-stable time (min) Graphene is combined |
| No. 1 | 25 | 54 |
| No. 2 | 25 | 46 |
| No. 3 | 25 | 42 |
A kind of zinc stearate/graphene oxide composite material for providing the present invention above and preparation method thereof has been carried out in detail
Thin introduction, specific case used herein is set forth to principle of the invention and implementation method, above example
Illustrate that being only intended to help understands the method for the present invention and its core concept, including best mode, and also cause this area
Any technical staff can put into practice the present invention, including manufacture and use any device or system, and the side for implementing any combination
Method.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, may be used also
Some improvement and modification are carried out with to the present invention, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The scope of patent protection of the present invention is defined by the claims, and may include those skilled in the art it is conceivable that other realities
Apply example.If these other embodiments have is not different from the structural element of claim character express, or if they
Including equivalent structural elements of the character express with claim without essence difference, then these other embodiments should also be included in
In the range of claim.
Claims (10)
1. a kind of zinc stearate/graphene oxide composite material, it is characterised in that including zinc stearate and be compounded in zinc stearate
The graphene oxide on surface.
2. zinc stearate/graphene oxide composite material according to claim 1, it is characterised in that the zinc stearate
It is sheet zinc stearate；
The thickness of the graphene oxide is 0.1~0.5nm；
The zinc stearate is 1000 with the mass ratio of the graphene oxide：(1~50).
3. zinc stearate/graphene oxide composite material according to claim 2, it is characterised in that the zinc stearate/
The piece footpath of graphene oxide composite material is 4~12 μm；
The thickness of the zinc stearate/graphene oxide composite material is 30~70nm.
4. a kind of preparation method of zinc stearate/graphene oxide composite material, it is characterised in that comprise the following steps：
A) by graphene oxide, organic solvent miscible with water and water by after dispersion, obtaining graphene oxide dispersion；
B after the graphene oxide dispersion for) obtaining above-mentioned steps and the mixing of zinc source, precursor solution is obtained；
C zinc stearate/graphene oxide is obtained after) precursor solution that above-mentioned steps are obtained is reacted with stearic acid to be combined
Material.
5. preparation method according to claim 4, it is characterised in that in the graphene oxide dispersion, graphite oxide
The mass fraction of alkene is 0.5 ‰~5 ‰；
The organic solvent miscible with water is included in alcohols solvent, amine solvent, ketones solvent and high molecular polymer solvent
One or more；
The mass ratio of the organic solvent miscible with water and water is (0.01~1)：1.
6. preparation method according to claim 4, it is characterised in that the zinc source is zinc source solution；
The concentration of zinc source solution is 0.01~0.5mol/L；
The zinc source includes one or more in zinc acetate, zinc chloride, zinc nitrate, zinc sulfate and zinc perchlorate；
The graphene oxide is 1 with the mass ratio of zinc ion in the zinc source：(1~10).
7. preparation method according to claim 4, it is characterised in that described to be mixed into ultrasonic disperse；
The temperature of the mixing is 20~60 DEG C；The time of the mixing is 10~60min.
8. the preparation method according to claim 4~7 any one, it is characterised in that the step C) it is specially：
To stearic acid organic solution is slowly added in the precursor solution that above-mentioned steps are obtained, stearic acid is obtained after being reacted
Zinc/graphene oxide composite material；
The stearic acid is (1.5~2.5) with the mol ratio of zinc ion in the zinc source：1；
The temperature of the reaction is 60~100 DEG C；The time of the reaction is 90~150min.
9. preparation method according to claim 8, it is characterised in that the concentration of the stearic acid organic solution is 0.1~
0.3mol/L；
Solvent in the stearic acid organic solution is included in alcohols solvent, benzene kind solvent, polynary alkanes solvent and ether solvent
One or more；
The speed being slowly added to is 0.3~0.7mL/s.
10. zinc stearate/the graphene oxide composite material or claim 5~9 times described in Claims 1 to 4 any one
Application of the zinc stearate/graphene oxide composite material anticipated prepared by rubber or resin additive field.
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| CN108854592A (en) * | 2018-06-14 | 2018-11-23 | 江苏大学 | Graphene oxide/isostearic acid composite separating film and its preparation method and application |
| CN109666198A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of graphene oxide enhancing rubber composite material and preparation method thereof |
| CN110964231A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Unsaturated carboxylic acid metal salt/graphene oxide composite material, preparation method thereof and functionalized graphene reinforced nitrile rubber |
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